Porous silicon nano-material and preparation method and use thereof

A nanomaterial and porous silicon technology, applied in the field of preparation of porous silicon nanomaterials, can solve the problems of harsh synthesis conditions, low yield, single Si quantum dots, etc., and achieve the effects of simple operation, high yield and high energy density

Active Publication Date: 2018-01-05
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method usually requires harsh synthesis conditions, the yield is very low, and generally only a single Si quantum dot can be obtained

Method used

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  • Porous silicon nano-material and preparation method and use thereof
  • Porous silicon nano-material and preparation method and use thereof
  • Porous silicon nano-material and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Step 1: Mix 1 mL of tri-n-propylamine and 1.1 mL of HSiCl 3 Add to 40 mL anhydrous CH 2 Cl 2 , stirred overnight at room temperature. Add 1 g Mg 2 Si (Mg 2 The scanning electron microscope pictures of Si are shown in figure 1 , lumpy solid, no particular shape), stirred and reacted at room temperature for 10 hours. Centrifuge, wash with chloroform 3-4 times, and dry in vacuo to obtain a brown solid.

[0041] Step 2: Put the obtained brown solid in a tube furnace with high-purity Ar gas at 15°C min -1 Heat at a heating rate of 700°C and hold for 30 minutes. After natural cooling, the obtained solid was washed with 1 M HCl, and then washed several times with distilled water, and dried in vacuum to obtain about 0.5 g (yield 74%) of yellow-brown porous silicon nanomaterials. figure 2 It is an X-ray powder diffraction pattern of the porous silicon nanomaterial, and it can be seen from the figure that the silicon material obtained by high temperature treatment is cr...

Embodiment 2

[0046] 1.1 mL HSiCl 3 Add to 40 mL anhydrous CH 2 Cl 2 , stirred overnight at room temperature. Add 1 g Mg 2 Si, the reaction was stirred at room temperature for 48 hours. centrifuged, washed 3-4 times with chloroform, and dried in vacuo, the gray solid obtained was unreacted Mg 2 Si and a small amount (about 20 mg, yield less than 10%) of Si nanoparticles. Compared with Example 1, in the absence of activator, porous silicon nanomaterials with mesoporous channels cannot be obtained.

Embodiment 3

[0048] Mix 1 mL of tri-n-butylamine and 1.1 mL of HSiCl 3 Add to 40 mL anhydrous CH 2 Cl 2 , stirred overnight at room temperature. Add 1 gMg 2 Si, the reaction was stirred at room temperature for 12 hours. Centrifuge, wash with chloroform 3-4 times, and dry in vacuo to obtain a brown solid.

[0049] The obtained brown solid was placed in a tube furnace with high-purity Ar gas at 15 °C min -1 Heat at a heating rate of 700°C and hold for 30 minutes. After natural cooling, the obtained solid was washed with 1 M HCl, and then washed several times with distilled water, and dried in vacuum to obtain about 0.5 g of yellow-brown crystalline porous silicon nanomaterials. The X-ray powder diffraction results of the porous silicon nanomaterial and figure 2 Basically the same. The nitrogen adsorption test results show that the specific surface area of ​​the material is 185 m 2 g -1 , showing distinct mesoporous channels (pore diameters around 3.5 nm and 25 nm). Referring to ...

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Abstract

The invention discloses a preparation method of a porous silicon nano-material. The preparation method comprises that chlorosilane and magnesium silicide undergo a reaction in an anhydrous organic solvent under action of an activator at the room temperature to 200 DEG C to produce the porous silicon nano-material having mesopores and a large specific surface area. Compared with the traditional synthesis method, the preparation method is easy to operate, has mild reaction conditions, has a high yield, easily realizes large-scale synthesis and has a low cost. After carbon coating treatment, theporous silicon nano-material can be used as a negative electrode material of a lithium-ion battery and has high energy density and excellent cycling performances.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a method for preparing porous silicon nanomaterials, that is, a porous silicon nanomaterial with mesopores and a large specific surface area is prepared by reacting metal silicide and chlorosilane in a solvent, and its application It can be used as negative electrode material of lithium ion battery or as molecular sieve material in the fields of adsorption, separation, catalysis and medical treatment. Background technique [0002] In recent years, lithium-ion batteries based on Si anode materials have received extensive attention, and the main advantage is that the theoretical capacity of Si anodes is greatly improved compared with traditional graphite anodes (~4000 mAh g -1 vs. ~370mAh g -1 ). However, the volume change of the Si negative electrode is greater than 300% during the process of intercalating and removing lithium, which leads to the fact that the active m...

Claims

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Application Information

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IPC IPC(8): C01B33/027H01M4/38H01M10/0525
CPCY02E60/10
Inventor 杜红宾孙林
Owner NANJING UNIV
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